Diisopropylethylamine → HCID 45142247, 화합물

HRID 875113

반응식

HRID 875113 반응식
[CH:1]1([NH:6][C:7]2[N:16]=[CH:15][C:14]3[CH2:13][CH2:12][C:11]4[C:17]([C:21]([O-])=[O:22])=[N:18][N:19]([CH3:20])[C:10]=4[C:9]=3[N:8]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[K+].C([N:27](C(C)C)C(C)C)C.N1(C([O-])=O)C2C=CC=CC=2N=N1.[NH4+]>CN(C)C=O.O1CCCC1.O>[CH:1]1([NH:6][C:7]2[N:16]=[CH:15][C:14]3[CH2:13][CH2:12][C:11]4[C:17]([C:21]([NH2:27])=[O:22])=[N:18][N:19]([CH3:20])[C:10]=4[C:9]=3[N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1

참가 물질

7

반응물 3

HCID 81531DiisopropylethylamineHCID 45140959Potassium 8-(cyclopentylamino)-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylateHCID 57454228HCID 57454228, 화합물

생성물 1

HCID 45142247HCID 45142247, 화합물수율 90%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

A suspension of potassium 8-(cyclopentylamino)-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate (180 mg, 0.51 mmol) in anhydrous dimethylformamide (3.0 mL) and anhydrous tetrahydrofuran (3.0 mL) was treated with N-ethyl-N,N-diisopropylamine (0.175 mL, 2 eq.) and N-ethyl-N′,N′-diisopropyl carbodiimide hydrochloride (EDCI) (195 mg, 2 eq). The mixture was then cooled to 0° C. and treated with ammonium 1H-1,2,3-benzotriazol-1-ate (137 mg, 2 eq). After 5 minutes the reaction was warmed to room temperature and kept at this temperature overnight. The reaction was diluted with water and the resulting precipitate was collected by filtration to afford the title compound (143 mg, 90% yield).

후처리

  1. temperatureAfter 5 minutes the reaction was warmed to room temperature
  2. customkept at this temperature overnight
  3. filtrationthe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-5b21b46642bf45828175aa9c412877c0
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08981089B2

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